関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Decalin | HCID 7044 | — |
| 反応物 | Dibenz(b,f)azepine | HCID 9212 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 4,4'-Diiodo-1,1'-biphenyl | HCID 76348 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 5-(4'-Iodobiphenyl-4-yl)dibenz[b,f]azepine | HCID 21311077 | 50% |
反応手順
5H-Dibenz[b,f]azepine in an amount of 20.0 g (0.10 mol), 4,4'-diiodobiphenyl in an amount of 60.9 g (0.15 mol), potassium hydroxide in an amount of 6.7 g (0.12 mol) and a copper powder in an amount of 1.3 g (0.02 mol) were mixed with 20 ml of decalin, and heated with stirring in a stream of nitrogen for 36 hours at the external temperature of 200° C. After cooling to room temperature or its vicinity, the reaction solution was admixed with chloroform, and subjected to Celite filtration to remove the insoluble matter. The filtrate was concentrated, and the concentrated solution was purified by column chromatography on silica gel. Thus, 23.6 g of 5-(4'-iodobiphenyl-4-yl)dibenz[b,f]azepine was obtained (in a 50% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05929235 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-92c8721821554ee5abeb0f6e915bc73b |
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| 出典メモ | uspto-grants-1999_07 |
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